Author Topic: Hydriodic Acid--Step by Step Write-Up  (Read 17012 times)

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Rhodium

  • Guest
You need a large excess of HI to reduce ...
« Reply #40 on: March 21, 2003, 02:14:00 PM »
You need a large excess of HI to reduce ephedrine, not just two equivalents - that is just the theoretical amount.

amalgum

  • Guest
right
« Reply #41 on: March 21, 2003, 02:48:00 PM »
Yeah your right, nothing is ever 100% efficient, esp. this type of rxn.  How much exactly of an excess are we talking about?  I would try to calculate it using the theoretical amount of HI produced by the rp/I2 method, but there are too many different ratio's for that reaction out there, it's hard to determine which is best.

fierceness

  • Guest
Rhodium: regarding sodium sulfite + I2 + H20
« Reply #42 on: March 23, 2003, 02:14:00 PM »
is there any way that the sodium sulfite method of producing HI will produce any extremely poisonous H2S in the process as a side reaction?

We dont want bees killing themselves trying to do this procedure

Rhodium

  • Guest
Redox chemistry of sulfur
« Reply #43 on: March 23, 2003, 02:53:00 PM »
As SO32- is itself the reducing agent acting on I2 in this case, that is highly unlikely, as that would mean SO32- could spontaneously disproportionate from S4+ (sulfite) to S2- (sulfide) and S6+ (sulfate), which it doesn't as S2- is oxidized to elemental sulfur by I2 - see

https://www.thevespiary.org/rhodium/Rhodium/chemistry/hydriodic.html


amalgum

  • Guest
more stuff
« Reply #44 on: March 24, 2003, 08:29:00 AM »
SWIM has procured new materials today.  After SWIM extracts the pseudo he will try a small rxn, and post results.

amalgum

  • Guest
first try
« Reply #45 on: March 28, 2003, 03:22:00 AM »
Alright, SWIM had 4g pseudo to start with.  To a 250mL rb flask, SWIM added 4g pseudo, 5g Na2SO3, 10g I2, and about 2mL of water.  The flask was stoppered with a glass tube sealed with a balloon.  SWIM shook the flask thoroughly to mix the shit.  At first it was just wet and clumpy.  SWIM added a little heat from a candle (not much, the flask was high above the candle), and the contents got liquidy, and started bubbling a little bit.  For the first 15-20, things went along pretty much like an rp rxn. After that, it pretty much died down a lot.  SO the flask was lowered closer to the candle.  After a few minutes, the shit started getting a lot more liquidy and bubbled more. The balloon also inflated pretty well.  It was allowed to go like this for another 20.  Then SWIM began to notice that a dark colored smoke appeared, that was kinda purplish, and looked like iodine subliming.  SWIM let it stay for about 5 minutes then took it off heat and swirled around really well.  SWIM let it cool until the balloon looked like it was gonna be sucked into the flask.  Then, it was removed, and about 1.5mL of h2o was added.  The balloon was replaced and the flask reheated.  The rxn eventually got hot enough to continue like before, so SWIM lowered the flask just a little more, and continued to boil for another 15 minutes or so.  Then the candle was blown out.
SWIM is awaiting the contents of the flask cool now, and is still unsure about the outcome of this rxn yet.  WIll keep updating.

amalgum

  • Guest
hrmmm
« Reply #46 on: March 28, 2003, 04:29:00 AM »
Well, SWIM did a water extract, then acidified with 6 drops of conc HCl and did a couple more extracts.  Looks to be a helluva lot of unreacted iodine left folks.  All the aqueous extracts had to be washed with xylene about 5 times before becoming devoid of most iodine.  SWIM has basified solution with NaOH.  A whole lot of freebase of something came out.  Although it did not have the look and feel of a completed rxn, nor quite the smell.  Looks like probably a bunch of unreacted pseudo.  Well, SWIM will go ahead with the a/b, and update.  If it didn't work, at least SWIM will have some pseudo back.

amalgum

  • Guest
fucking shit
« Reply #47 on: March 29, 2003, 06:17:00 AM »
Well, the rxn was definietly a failure.  SWIM doesn't think that a "dry" type reaction will work at all.  Even though the theorhetical amount of H2O was present, the mixture still seemed pretty dry, and almost no reaction was evident.  SWIM thinks in order for the Na2SO3/I2 reaction to succesfully produce HI, an excess of water is needed.  In the "dry" run, the sublimation of iodine inside was noticeable, and at the end it seemed like almost no I2 had reacted.  SWIM did another test with the Na2SO3/I2 thing again.  SWIM did it like the first little test, added a small amount of Na2SO3 to a beaker, the right amount of I2, and a huge excess of water (enough to submerge everything).  Like before, upon a little heating, it seemed almost all the iodine immediately dissolved (the rest like 2 seconds later), and the smell of HI was apparent.  After about five minutes, no apparent elemental iodine was detected.

So this leads SWIM to the conclusion that in order for this to work it must be a reflux reduction.  SWIM went ahead and used the recovered pseudo  (what was left anyway) in a normal rp/I2 for now.
In a little bit, when SWIM gets more funds, a reflux will be tryed.  Psuedoephedrine will be dissolved in a minimal amount of dH2O.  Reflux apparatus will be setup, and Na2SO3 and I2 will be added.  Then SWIM will reflux mixture for about 3-4 hours.  By that time, depending on how things are going (this of course would be a small amount for testing, like 2-4g pseudo), SWIM will decide whether or not he should add more Na2SO3/I2 and continue for another few hours, or proceed with workup.  Either way, SWIM will probably reflux at minimum 6 hours for starters, keeping HI conc. up of course.

hermanroempp

  • Guest
Wrong pH perhaps?
« Reply #48 on: March 29, 2003, 05:22:00 PM »
I think the reaction needs to be done under acidic conditions. The equation

Na2SO3 + I2 + H2O --> Na2SO4 + 2 HI

looks good on paper, but in the real world another reaction like

Na2SO3 + I2 + H2O --> NaHSO4 + HI + NaI

will also occur. However, the truth is somewhere in between those two reaction paths  :) ....depending on pH, amount of solvent(read: water), temperature etc.
My 2 cents: If the solution of sodium sulfite is acidified prior to reaction (with a non-oxidizing acid, of course) to yield a solution of free H2SO3, and then the iodine is reacted with the acid solution, then a solution of HI will form. But I think the solution of HI will be too diluted to be directly employed in a reduction, it must be concentrated via distillation  ::)


ahgreich

  • Guest
Whoo doggies. Success.
« Reply #49 on: April 08, 2003, 09:54:00 PM »
He's now feeling the product of a successful reduction of Pfed fb with
sodium sulfite,
iodine,
and dh20.

Phan-fucking tastique!!
No RP. Had to happen. It's all in the metaphysics, the incantations, and a few dead chickens.

Swim'll speak in equivalencies instead of empirical weights, as he don't have a scale.
in a 250 ml rbf, he placed the following, in order:

3 teaspoons of very dry, very clean pfeb fb xtals ( slightly over 3gms) pre-sifted with 6 teaspoons of sodium sulfite.
1 1/2 teaspoons of dh20 on the top of the dry pile at bottom of flask (enough that the whole pile was wet enough to sling about, yet not thin - consistency of black-strap molasses.

He then 'staged' around 11g I in a small beaker, readied  his punch baloon: dumped in the I, snaped the balloon on top, taped the hell out of it, and waited.

20 sec or so, exotherm began without addition of ANY external heat source.

pile got nasty purple, bubbling. NO SMOKE. He watched it for about 10 minutes until the I had been reacted (no longer a purple nasty mass, but light pale beige-ish. No smoke yet, no balloon movement inflation. bubbling subsided.

On to the stove he went, appling liberal heat such that the punch balloon was the size of a large grapefruit. The flask contents evolved a brilliant yellow. Removed from heat, watched some clear liquid run down flask neck, waited for flask to cool (15 minutes or so) - the pasty flask contents became white as it cooled. At room temp, was nearly as white as sodium sulfite. All the while, he was fondling the flask, rolling it, jiggling it, keeping the liquid moving.

Back to the stove, heat until boil and balloon inflated, contents turned back yellow! Removal from heat and close observation revealed that the contents where getting shiny-like.

Did this routine 3 times, each time yellow when hot, white when cool.

last time cool, removed balloon, no smoke, didn't stick his nose in for a smell - strange really, no strong smells to speak of during the whole party. The strong-ass punchy was secured on the flask before any reaction started, retaining all gas.

workup - 2 tolly washes of post rxn b4 basing into 3rd shot of tolly with
Ass-load of NaOH (he reckons to polarity-crawl back through the aq NaSO4 (from the sodium sulfate rxn product).

Should have washed the tolly with base a few more times, however, as he is sailing through the bioassay:
HCL/dH20 xtylzation - exceptional. Da real medicine, all nice like.
long legs, slight whitish residue (see prior sentence about washing NP better prior to HCL/H20).


RP/I smells not noticable during the endeavor.

Why did it succeed? He thinks:
1. JUST enough dH20 to have high enough concentration of aqHI as HI was generated yet not so much that ALL of the HI would have a place to go as soon as it was made.
3. application of heat meant that the HI concentration in dH20 was affected causing the yellowing. However, the heat facilitated the mobility of the flask contents, at times becoming a true reflux.


Whooeeee. How bout them apples?

ballzofsteel

  • Guest
Well done dude, Not to be a knocker,as I think
« Reply #50 on: April 09, 2003, 12:18:00 AM »
Well done dude,

 Not to be a knocker,as I think it is brilliant that you have explored un-trodden ground and reported a successful reaction,which,If true holds many possibilities for all of us,
Butt...I feel you owe it to yourself to bring some credibility to your experimental results by composing a complete write-up,with accurate measurements etc.
This will help other, less forgiving bees believe and share in your enjoyment.
Please replicate and document this for me.

Good work dude.

Organikum

  • Guest
thats true new
« Reply #51 on: April 09, 2003, 07:47:00 AM »
and beats the shit out of every phosphor(o)us reaction in availability of needed chems.
Ballz, ahgreich has no scale and for me are accurate teaspoon measurements as good as mikrograms.

so thanks ahgreich!  ;D
Please report further success as misfortune on this - I am eager to hear more!

ORG


RepVip

  • Guest
ahgreich - more info please
« Reply #52 on: April 12, 2003, 06:26:00 PM »
In reference to

Post 399133

(Rhodium: "New ways for making HI", Stimulants)

and

Post 424974

(ahgreich: "Whoo doggies. Success.", Stimulants)


ahgreich can you please provide more info on your "successful" experiment? I'm surprised you didn't use a scale. Unless you are intimately aquainted with iodine and sodium sulfite, 'staging' accurate amounts is really, really difficult. A pinch of this and a dash of that just isn't going to cut it.

It's hard not to be a critic - it sounds too good to be true! And you know what they say... Please prove me wrong!! This method seems one of the best yet - if it works.

Anybees with more information please post! I'd experiment myself, but I'm lacking a few chems. However, I'll be forced to if nobee does  :)

ropoctl

  • Guest
Acidified SO 3 2- is SO2(g).
« Reply #53 on: July 28, 2003, 08:23:00 PM »
Acidified SO32- is SO2(g).  The species H2SO3 does not exist, just as H2CO3 or NH4OH cannot be isolated.

bloosh

  • Guest
can you please help me ?
« Reply #54 on: February 10, 2004, 06:22:00 PM »

NMR

  • Guest
There is a much easier, faster, and cheaper way
« Reply #55 on: October 31, 2004, 08:09:00 AM »
The phosphoric/iodide reaction is good in that it uses non watched ingredients, but it requires extensive glassware, a heating mantel and considerable time to complete.
   The second method that you outline is the preferred method, that is, the hydrogen sulfide method; it is fast, it is cheaper than the above method, and it requires no special equipment or facilities.
   I will quickly outline it as follows:

   This method requires three ingredients: hydrogen sulfide gas, elemental iodine, and water.

1.   Iodine is procured as usual or may be obtained from the potassium iodide used in the other author's reaction by treating an aqueous solution of potassium iodide with a small amount of concentrated sulfuric acid to first convert the iodide and then by adding slowly with much stirring sodium hypochlorite solution to form chlorine gas insitu to force the crystalline iodine out of solution.  The iodine thus formed may be filtered for further use.

2.   Hydrogen sulfide gas is formed and bubbled into a flask containing crystalline iodine from above and water with constant stirring and or swirling.  When the reaction is complete one will have a clear liquid, also known as aqueous HI with a spongy yellow wad of sulfur in the bottom of the flask.  Simply pick out the spongy sulfur wad and throw it away and you are done; you now have fresh, crystal clear, concentrated HI, for use in doing whatever.

3.   Hydrogen sulfide gas is formed by dropping a chunk of ferrous sulfide into a weak solution of any acid that you might have available and piping the gas to the bottom of the container containing the iodine and water, just like any other gassing operation that you are familiar with.

4.   Ferrous sulfide is very easily and cheaply made in unlimited quantities, here is an example synthesis:
   1. Weigh out 1 mole (32.1 grams) of Sulfur, purchased in any garden supply store or hardware store.
   2. Weigh out 1 mole (55.85 grams) of Iron filings or Super Fine Steel Wool Pads if you can't find the iron filings purchased at a hardware store.
   3. Combine the two above ingredients in a large stainless steel cooking pot with a good fitting lid.
   4. Add one half gallon of water, less if filings are used because they are more compact than the puffy steel wool pads.  Make sure that the pads are covered completely, add more water if necessary to cover the pads.
   5. Bring to a boil and boil until dry.  The reaction begins rather quickly, you will notice that the pads become quite black and the water becomes black.  Since a faint odor of sulfide is given off during boiling and conversion, a good stove top exhaust fan is a must.  After half an hour or so, if convenient, finish off the boiling to dry outside, say, on a barbeque grill.
   6.  When boiled dry, you will have enough ferrous sulfide to make enough hydrogen sulfide to make a half gallon of acid.

STORE ANY UNUSED FERROUS SULFIDE IN AN AIR TIGHT CONTAINER, AS IT SLOWLY REACTS WITH AIR AND MOISTURE TO GIVE OFF SMALL QUANTITIES OF HYDROGEN SULFIDE GAS.  BEST TO STORE IT OUTSIDE IN A TOOL SHED OR IN SOME OTHER WELL VENTILATED PLACE UNLESS STORED IN A VERY AIRTIGHT CONTAINER.
HYDROGEN SULFIDE IS A POISONOUS GAS, MAKE THE GAS AND USE IT OUTSIDE AND STAY UP WIND, DO NOT BREATH IT, IT SMELLS LIKE ROTTEN EGGS, SO YOU CAN'T MISS IT, BE CAREFUL.

ONCE THE PRECURSOR IS MADE, THE TIME TO MAKE THE ACID IS LESS THAN AN HOUR, NO HEAT REQUIRED, IT IS DONE AT ROOM TEMPERATURE, NO MUSS, NO FUSS.

Zen

  • Guest
A+ Write Up (HI the right way.)
« Reply #56 on: October 31, 2004, 09:47:00 PM »
Nice procedure and no high explosives.

Easy does it, make sure you have tight seals, poisonous gases can make you unhappy.

Awesome write up NMR. 8)

Lestat

  • Guest
I like it, nice and simple HI, I just want to...
« Reply #57 on: November 01, 2004, 01:23:00 AM »
I like it, nice and simple HI, I just want to add a couple of things, about H2S, it is HIGHLY toxic, problem is, if you inhale sublethal amounts, it quickly knocks out your sense of smell, causing the would-bee chemist to beelieve the H2S has dissipated and causing said chemist's removal from the gene pool :o

And dropping ferrous sulfide into an acid works, but dripping the acid SLOWLY onto the sulfide is a much safer way of going about things so as to avoid a runaway reaction and generation of overlarge amounts of H2S from beeing possible :)

Another way, SWIM uses occasionally to generate H2S, is to mix candle wax and sulfur powder and heat, this generates quite considerable amounts of H2S, although likely there is a fair amount of volatilised S vapor, and a little SO2 assuming the heating/gassing setup hasn't firsthand been purged of oxygen.

When working with H2S I advise a scrubbing setup to bee put in place, with a tank full of something for surplus H2S to reduce, preferably one that would produce a possibly useful reagent, or ammonia solution.

If you used NH3 solution, then perhaps you could get into selling stinkbombs as a little side-earner, as ammonium sulfides smell rather foul. Stinkbombs made with it are quite certainly effective ;)


Scottydog

  • Guest
Water Ratio?
« Reply #58 on: November 01, 2004, 02:03:00 AM »
The method seems fairly self explanatory but lacking in one minor detail.

"2. Hydrogen sulfide gas is formed and bubbled into a flask containing crystalline iodine from above and water with constant stirring and or swirling.  When the reaction is complete one will have a clear liquid, also known as aqueous HI with a spongy yellow wad of sulfur in the bottom of the flask.  Simply pick out the spongy sulfur wad and throw it away and you are done; you now have fresh, crystal clear, concentrated HI, for use in doing whatever."

What is the proper water ratio in relation to weight of iodine to bee gassed?

I suppose a push/pull with a NaOH solution might work to eliminate excess H2S gas?

Might make for a good "theoretical" camping project. SWIM likes the idea of dropping the FeS into the dilute acid to produce the H2S gas. Could actually bee self-supervising! Drop in the precursor, affix the stopper and then leave for a few hrs, returning later to the HI solution that only requires a filtering of the sulfur.

Great followUP!


Zen

  • Guest
scrubbing setup
« Reply #59 on: November 01, 2004, 02:51:00 AM »
A scrubber is good idea # 2.

H2S isn't very soluble in water.

psst.. you can also bubble hydrogen through
 iodine solution and "mysterious catalyst" to yield HI
 most effectively, but this works too.